Abstract
We report the synthesis, isolation, and structural characterization of an elusive organobismuth(III) dihydride (Ar*-Bi(III)-H(2), 1). The complex features a bulky and rigid (t)Bu-M(s)Fluind ligand that permits complete spectroscopic characterization and SC-XRD. The compound is thermally unstable and decomposes to quantitatively form H(2) and Ar*-Bi(I) in a chemoselective intramolecular process. In addition to H(2) formation, the presence of a Bi-H bond is supported by comparative spectroscopy (NMR and IR) with its deuterated analogue 1-d(2).